CN102992812B - Microcrystal-reinforced transparent leadless fritted glaze and preparation method thereof - Google Patents
Microcrystal-reinforced transparent leadless fritted glaze and preparation method thereof Download PDFInfo
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Abstract
本发明公开了一种微晶增强透明无铅熔块釉极其制备方法，属于陶瓷釉料加工领域。本发明制备的微晶增强透明无铅熔块釉，其化学成分质量百分比组成为：SiO2 45.0～55.0%、Al2O3 5.0～7.0%、Fe2O3 0.1～0.2%、CaO 2.0～11.0%、MgO 1.0～1.5%、K2O 2.0～4.0%、Na2O 0.5～2.0%、Li2O 0～3.0%、ZnO 7.0～9.0%、BaO 3.0～5.0%、SrO 2.0～2.6%、B2O3 5.0～10.0%、ZrO2 3.0～6.0%、La2O3 0～1.0%。采用碱金属、碱土金属和少量的稀土元素的复合熔剂代替熔块釉中的铅元素，铅溶出量为零，彻底解决了骨质瓷为代表的高档日用瓷中铅对人体的危害，制备得到的产品釉面光泽度好，透明度高，热稳定性好。The invention discloses a preparation method of a microcrystalline reinforced transparent lead-free frit glaze and belongs to the field of ceramic glaze processing. The microcrystalline reinforced transparent lead-free frit glaze prepared by the present invention has the following chemical components in mass percent: SiO 2 45.0-55.0%, Al 2 O 3 5.0-7.0%, Fe 2 O 3 0.1-0.2%, CaO 2.0- 11.0%, MgO 1.0～1.5%, K 2 O 2.0～4.0%, Na 2 O 0.5～2.0%, Li 2 O 0～3.0%, ZnO 7.0～9.0%, BaO 3.0～5.0%, SrO 2.0～2.6% , B 2 O 3 5.0-10.0%, ZrO 2 3.0-6.0%, La 2 O 3 0-1.0%. The composite flux of alkali metal, alkaline earth metal and a small amount of rare earth elements is used to replace the lead element in the frit glaze, and the amount of lead dissolution is zero, which completely solves the harm of lead in high-grade daily-use porcelain represented by bone china to the human body. The obtained product has good glaze gloss, high transparency and good thermal stability.
Description
Technical field
The invention belongs to ceramic glaze processing technique field, relate to a kind of crystallite and strengthen extremely preparation method of transparent lead-free fritted glaze.
Background technology
Pengyang china stone take Bone China, steatite ceramic, quartz enriched porcelain etc. as representative is with its beautiful outward appearance and good internal performance, very popular.These potteries generally adopt double-firing process, i.e. high temperature biscuiting, low temperature sinter.
As the glaze of these materials, the past is mostly used leaded fritted glaze, and leaded fritted glaze has that glossiness is high, melt temperature is low, firing range is wide, specific refractory power is high, low cost and other advantages, and leaded low temperature frit glaze is widely used.But, leaded fritted glaze has certain plumbous stripping, along with improving constantly of people's living standard, the degree of depth day by day healthy, environment is paid close attention to, ceramic glaze is produced and had higher requirement, the numerous and confused use of formulating the heavy metal elements such as the plumbous cadmium of more strict criteria limit of many countries.Prepare and do not use plumbous fritted glaze, both protected people's health, also improved production environment, fundamentally eliminated plumbous various harm, have broad application prospects.
In recent years, Some Enterprises is carrying out the research without lead frit always, has obtained some achievements, but ubiquity temperature of glaze firing is high, the problem such as low or low in glossiness of hardness of glaze surface.The problems the such as especially twice firing of the high-grade domestic ceramics take Bone China as representative (low temperature sinter) product ubiquity hardness of glaze surface is low, thermostability is good not, can not meet the requirement of cutlery to hardness of glaze surface performance.So preparing at low temperatures the nontoxic fritted glaze of high rigidity, good thermal stability is the task of top priority.
Summary of the invention
The problem that the present invention solves is to provide a kind of crystallite to strengthen transparent lead-free fritted glaze and preparation method thereof, adopts unleaded composite fluxing agent and the combination of crystallizing agent material, is a kind of low temperature high-hard, transparent lead-free fritting enamel of the glaze system that is applicable to many porcelain kind.
The present invention is achieved through the following technical solutions:
A kind of crystallite strengthens transparent lead-free fritted glaze, in massfraction, comprises following component: SiO
245.0～55.0%, Al
2o
35.0～7.0%, Fe
2o
30.1～0.2%, CaO 2.0～11.0%, MgO 1.0～1.5%, K
2o 2.0～4.0%, Na
2o 0.5～2.0%, Li
2o 0～3.0%, ZnO 7.0～9.0%, BaO 3.0～5.0%, SrO 2.0～2.6%, B
2o
35.0～10.0%, ZrO
23.0～6.0%, La
2o
30～1.0%.
A kind of crystallite strengthens transparent lead-free fritted glaze, in massfraction, by following material component, is fired and is formed:
Potassium felspar sand 18～28%, talcum 3～4%, borax 0～7%, boric acid 3～15%, Quilonum Retard 0～6%, calcium carbonate 3～17%, zinc oxide 6～9%, barium carbonate 2～6%, Strontium carbonate powder 2～4%, aluminium hydroxide 1～3%, lanthanum trioxide 0.2～1%, quartz 20～30%, zirconium silicate 2～8%.
Further, described in massfraction, by following material component, fire and form:
Potassium felspar sand 18～28%, talcum 3.17～4%, borax 1～7%, boric acid 3～15%, Quilonum Retard 2～6%, calcium carbonate 3～17%, zinc oxide 6～9%, barium carbonate 2～6%, Strontium carbonate powder 2～4%, aluminium hydroxide 1～3%, lanthanum trioxide 0.2～1%, quartz 20～30%, zirconium silicate 2～8%.
Crystallite strengthens a preparation method for transparent lead-free fritted glaze, comprises the following steps:
In massfraction, get following material component and fully mix:
Potassium felspar sand 18～28%, talcum 3～4%, borax 0～7%, boric acid 3～15%, Quilonum Retard 0～6%, calcium carbonate 3～17%, zinc oxide 6～9%, barium carbonate 2～6%, Strontium carbonate powder 2～4%, aluminium hydroxide 1～3%, lanthanum trioxide 0.2～1%, quartz 20～30%, zirconium silicate 2～8%;
After mixing, 1350～1450 ℃ of meltings, the fusion time is 180～250min, then after shrend, makes lead-free fritting enamel.
Describedly also take water as medium, add suspension agent polyacrylamide, lead-free fritting enamel ball milling in ball mill is made to glaze slip, the mass ratio that glaze slip fineness is controlled at 250 mesh screen residues is 0.02～0.05%.
The add-on of described suspension agent polyacrylamide is 0.15～0.25% of lead-free fritting enamel quality.
Describedly also glaze slip is imposed on the biscuit of ceramics of biscuiting, after 1150～1180 ℃ of glaze firing, obtain ceramic.
Compared with prior art, the present invention has following useful technique effect:
Crystallite provided by the invention strengthens transparent lead-free fritted glaze, adopt the composite fluxing agent of basic metal, alkaline-earth metal and a small amount of rare earth element to replace the lead element in fritted glaze, lead release is zero, the plumbous harm to human body in the high-grade household china that thoroughly to have solved Bone China be representative, can be good at adapting to the high-grade domestic ceramics base substrate take Bone China as representative.
Crystallite provided by the invention strengthens transparent lead-free fritted glaze, by devitrified glass enhancement techniques, after being imposed on base substrate, glaze slip carries out glaze firing, and in glaze firing process, glaze is separated out small high rigidity crystal, hardness of glaze surface is improved, has met the requirement of cutlery to hardness of glaze surface performance.And the product glaze obtaining is smooth, the crystallite dimension size that glaze chromatography goes out, for 100nm～300nm, is less than visible wavelength (390nm～780nm), obtains clear frit glaze, and hardness of glaze surface>=630Kgf/mm
2.
Crystallite provided by the invention strengthens transparent lead-free fritted glaze, can obtain good glaze quality, and the product glaze glossiness after burning till is good, and transparency is high, Heat stability is good; And overcome the defect that ceramic glaze temperature of glaze firing is high.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
Crystallite provided by the invention strengthens transparent lead-free fritted glaze, adopts the composite fluxing agent of basic metal, alkaline-earth metal and a small amount of rare earth element to replace the lead element in fritted glaze.In order better to control the quality of product, the chemical constitution of each raw material of prepared fritted glaze is in Table 1, and wherein the purity of industrial chemicals is more than 98%.
Table 1 raw material chemical constitution (wt%)
Embodiment 1:
Crystallite strengthens the preparation method of transparent lead-free fritted glaze, comprises the following steps:
Crystallite strengthens transparent lead-free fritted glaze, takes by mass percentage following desired raw material: potassium felspar sand 18.06%, borax 6.83%, talcum 3.17%, boric acid 3.23%, Quilonum Retard 2%, Strontium carbonate powder 3.03%, calcium carbonate 15.92%, zinc oxide 7%, barium carbonate 4.53%, aluminium hydroxide 4.18%, lanthanum trioxide 0.5%, zirconium silicate 4.57%, quartz 28.42%;
Each component raw material is mixed, in Cinker clew furnace, with the melt temperature melting 180min of 1400 ℃, after shrend, make lead-free fritting enamel;
Take water as medium, add 0.15% polyacrylamide of lead-free fritting enamel quality, lead-free fritting enamel ball milling in ball mill is made to glaze slip, glaze slip fineness is controlled at remaining (250 mesh screen residue) 0.02～0.05% of 10000-hole sieve;
Glaze slip is imposed on the Bone China biscuit of high temperature biscuiting, and then, through being fired into product, temperature of glaze firing is 1150 ℃.The ceramic product glaze obtaining is smooth, and glossiness test can reach 98%, and glaze chromatography goes out small crystal, and its size is 100nm～300nm, is less than visible wavelength (390nm～780nm), obtains clear frit glaze, and hardness of glaze surface>=630Kgf/mm
2.
Embodiment 2:
Crystallite strengthens the preparation method of transparent lead-free fritted glaze, comprises the following steps:
Take by mass percentage following desired raw material: potassium felspar sand 20.06%, borax 5%, talcum 3.17%, boric acid 8.97%, Quilonum Retard 2%, Strontium carbonate powder 3.03%, calcium carbonate 15.92%, zinc oxide 7%, barium carbonate 4.53%, aluminium hydroxide 1%, lanthanum trioxide 0.5%, zirconium silicate 4.57%, quartz 24.25%;
Each component raw material is mixed, in Cinker clew furnace, with the melt temperature melting 250min of 1450 ℃, after shrend, make frit;
Take water as medium, add 0.20% polyacrylamide of lead-free fritting enamel quality, frit ball milling in ball mill is made to glaze slip, glaze slip fineness is controlled at 10000-hole sieve and Yus 0.02～0.05%.
Glaze slip is imposed on the Bone China biscuit of high temperature biscuiting, and then, through being fired into product, temperature of glaze firing is 1160 ℃.The product glaze obtaining is smooth, and glossiness test can reach 98%, and glaze chromatography goes out small crystal, and its size is 100nm～300nm, is less than visible wavelength (390nm～780nm), obtains clear frit glaze, and hardness of glaze surface>=630Kgf/mm
2.
Embodiment 3:
Crystallite strengthens the preparation method of transparent lead-free fritted glaze, comprises the following steps:
Take by mass percentage following desired raw material: potassium felspar sand 25.06%, borax 1%, talcum 3.17%, boric acid 14.65%, Quilonum Retard 6%, Strontium carbonate powder 3.03%, calcium carbonate 3.86%, zinc oxide 7%, barium carbonate 4.53%, aluminium hydroxide 1%, lanthanum trioxide 0.5%, zirconium silicate 6.84%, quartz 26.15%;
Each component raw material is mixed, in Cinker clew furnace, with the melt temperature melting of 1450 ℃, after shrend, make frit;
Take water as medium, add 0.25% polyacrylamide of lead-free fritting enamel quality, frit ball milling in ball mill is made to glaze slip, glaze slip fineness is controlled at 10000-hole sieve and Yus 0.02～0.05%.
Glaze slip is imposed on the Bone China biscuit of high temperature biscuiting, and then, through being fired into product, temperature of glaze firing is 1180 ℃.The product glaze obtaining is smooth, and glossiness test can reach 98%, and glaze chromatography goes out small crystal, and its size is 100nm～300nm, is less than visible wavelength (390nm～780nm), obtains clear frit glaze, and hardness of glaze surface>=630Kgf/mm
2.
The chemical constitution of the prepared lead-free fritting enamel of above-described embodiment 1-3 is as shown in table 2.
The chemical constitution (wt%) of table 2 embodiment
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| SiO 2 | 51.48 | 48.64 | 52.38 |
| Al 2O 3 | 6.71 | 5.94 | 6.81 |
| Fe 2O 3 | 0.09 | 0.11 | 0.12 |
| CaO | 10.66 | 10.81 | 2.56 |
| MgO | 1.22 | 1.24 | 1.18 |
| K 2O | 2.79 | 3.13 | 3.69 |
| Na 2O | 1.73 | 1.44 | 0.72 |
| Li 2O | 0.96 | 0.97 | 2.75 |
| ZnO | 8.30 | 8.40 | 7.91 |
| BaO | 4.17 | 4.23 | 3.98 |
| SrO | 2.53 | 2.56 | 2.41 |
| B 2O 3 | 5.11 | 8.25 | 9.73 |
| ZrO 2 | 3.64 | 3.69 | 5.20 |
| La 2O 3 | 0.59 | 0.60 | 0.56 |
Claims (6)
1. crystallite strengthens a transparent lead-free fritted glaze, it is characterized in that, in massfraction, comprises following component: SiO
245.0～55.0%, Al
2o
35.0～7.0%, Fe
2o
30.1～0.2%, CaO2.0～11.0%, MgO1.0～1.5%, K
2o2.0～4.0%, Na
2o0.5～2.0%, Li
2o0～3.0%, ZnO7.0～9.0%, BaO3.0～5.0%, SrO2.0～2.6%, B
2o
35.0～10.0%, ZrO
23.0～6.0%, La
2o
30～1.0%.
2. crystallite strengthens a transparent lead-free fritted glaze, it is characterized in that, in massfraction, by following material component, is fired and is formed:
Potassium felspar sand 18～28%, talcum 3～4%, borax 0～7%, boric acid 3～15%, Quilonum Retard 0～6%, calcium carbonate 3～17%, zinc oxide 6～9%, barium carbonate 2～6%, Strontium carbonate powder 2～4%, aluminium hydroxide 1～3%, lanthanum trioxide 0.2～1%, quartz 20～30%, zirconium silicate 2～8%.
3. crystallite as claimed in claim 2 strengthens transparent lead-free fritted glaze, it is characterized in that, in massfraction, by following material component, is fired and is formed:
Potassium felspar sand 18～28%, talcum 3.17～4%, borax 1～7%, boric acid 3～15%, Quilonum Retard 2～6%, calcium carbonate 3～17%, zinc oxide 6～9%, barium carbonate 2～6%, Strontium carbonate powder 2～4%, aluminium hydroxide 1～3%, lanthanum trioxide 0.2～1%, quartz 20～30%, zirconium silicate 2～8%.
4. crystallite strengthens a preparation method for transparent lead-free fritted glaze, it is characterized in that, comprises the following steps:
In massfraction, get following material component and fully mix:
Potassium felspar sand 18～28%, talcum 3～4%, borax 0～7%, boric acid 3～15%, Quilonum Retard 0～6%, calcium carbonate 3～17%, zinc oxide 6～9%, barium carbonate 2～6%, Strontium carbonate powder 2～4%, aluminium hydroxide 1～3%, lanthanum trioxide 0.2～1%, quartz 20～30%, zirconium silicate 2～8%;
After mixing, 1350～1450 ℃ of meltings, the fusion time is 180～250min, then after shrend, makes lead-free fritting enamel;
Also, take water as medium, add suspension agent polyacrylamide, lead-free fritting enamel ball milling in ball mill is made to glaze slip, the mass ratio that glaze slip fineness is controlled at 250 mesh screen residues is 0.02～0.05%; The add-on of described suspension agent polyacrylamide is 0.15～0.25% of lead-free fritting enamel quality.
5. crystallite as claimed in claim 4 strengthens the preparation method of transparent lead-free fritted glaze, it is characterized in that, in massfraction, gets following material component and fully mixes:
Potassium felspar sand 18～28%, talcum 3.17～4%, borax 1～7%, boric acid 3～15%, Quilonum Retard 2～6%, calcium carbonate 3～17%, zinc oxide 6～9%, barium carbonate 2～6%, Strontium carbonate powder 2～4%, aluminium hydroxide 1～3%, lanthanum trioxide 0.2～1%, quartz 20～30%, zirconium silicate 2～8%.
6. crystallite as claimed in claim 4 strengthens the preparation method of transparent lead-free fritted glaze, it is characterized in that, also glaze slip is imposed on the biscuit of ceramics of biscuiting, after 1150～1180 ℃ of glaze firing, obtains ceramic.
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Granted publication date: 20140416 Termination date: 20211204 |